Field of the Invention

The p resent invention relates to a cold and hot process of structu ring of cosmetic compositions . More specifically, the present invention relates to a process for the preparation of cosmetic compositions , in that, initially organogels are prepared , which besides the usual components such as organic liquids to be structured and structuring agents, are added natural or synthetic polymers and/or polyol esters. Thus, the organogels prepared are the base for cold and hot process of structuring cosmetic compositions upon the add ition of water, aqueous solutions or other active components or not.

Background of the invention

Emulsions

Em ulsions are dispersed systems consisting of two immiscible liqu id phases (oil and water) , where the dispersed or internal phase is finely d ivided and distributed in another external or continuous phase.

The conventional emulsions are classified in oil/water (O/W) when the oil droplets are dispersed in water and water/oil (W/O) , when water d roplets are dispersed In oil . It is important to clarify that by "oil" is considered all nonpoiar hydrophobic liquids and by "water" is considered all highly polar hydrophilic liquids,

In principle , oil and water phases are made up of only one substance, however, in cosmetic preparations, each phase usually contains a variety of "components". The viscosity of the emulsion and its appearance are controlled, in part, by the type of emulsion , the particle size of the dispersed phase and the ratio between the internal and external phases. The system is thermodynamically u nstable: the particle size can vary once the internal phase constantly tries to agglomerate and separate forming a second phase.

Polymers and emulsifiers are used to delay this inevitable separation . Du ring the process of the emulsion formation , these compounds can be adsorbed in the oil-water or water-oil interface. Depend ing upon the agent used and by the reduction of interfaclal tension , it promotes the stabilization of finely divided d roplets and controls the type of em ulsion formed (W/O or O/A) . Organogels

Orga nogels are defined as thermoreversible th ree-d imensional gel network that immobilizes a n organic fluid creating a material with characteristics and rheological properties of a solid , but with g reater part of its composition being liquid . They can also be defined as a viscoelastic material composed by a structuring agent and a nonpolar liq uid phase . They are semisolid systems where an oil phase is immobilized by a self-assembled three dimensional network formed by the structuring agent, The liquid phase may be a polar organic solvent (such as benzene, hexane, etc. ) , mineral oil or vegetable oil.

Several chemical compounds are able to structure organ ic liquids forming organogels. Some examples are 12-hydroxystearic acid, sterols, lecithins, mono- and diglycerides, lecithin m ixtures with sorbitan esters, fatty acids and fatty alcohols and waxes and wax esters .

The potential applications of organogels in food , pharmaceutical, cosmetic and petrochemicals ind ustries have raised the interest in this type of material . The interest is partly d ue to the great diversity of possible mesoscopic and microscopic structu res, In the fooa ind ustry there is a great potential for the use of organogels. It can be used to min imize oil migration i n food with multiple components, for example, chocolates. Can also be used to structure edible oils, consequently red ucing the use of saturated and trans fat. The organogel technology has also been applied in the pharmaceutical field to structure dermal and transdermal products and as transporter or carrier system for topical d rugs or therapeutic substances. I n the petrochemical ind ustry there are investigations to study the possibility to contain oil spills using gelation phase of the selective organogels , a nd also gelation of flammable solvents for storage and transportation . They have been also used in the preservation of works of art, where the solvents used to clean oil paintings are gelled in order to prevent its penetration in original layers of paint and prevent damage to the work.

The structu ring of oil has recently been applied in the cosmetic industry as structurers for personal care products . It is also known that waxes are applied in structuring oily bases for lipstick, "gloss", eyeliners, lip balms, etc. Structured emulsions are part of a different scope of organogels. These emulsions refer to structured oils by structuring agents, which, d ue to their amphiphil'c natu re, allow the incorporation of a significant amount of water. Brief Descri ptio n of the Figures

The illustrative figures attached , shows the m icrographs of examples of cosmetic compositions according to the present invention . It should be considered , however, that such illustrations do not serve to lim it or define the overall scope of the invention . The figures are;

FI GU RE 1 - Polarized Light Microscopy of an emulsion prepared from Organogel 1 (3%) in water (97%) . Oil in water emulsion (O/W) .

FI G U RE 2 - Optical microscopy of an emulsion prepared from Organogel 1 (3%) in water (97%) . Oil in water emu lsion (O/W).

FI G URE 3 - Optical microscopy of an emulsion prepared from

Organogel 2 (3%) in water (97% ). Lamellar em ulsion .

FIG URE 4 - Optical microscopy of the emulsion prepa red from Organogel 3 (3 %) in water (97%). Lamellar emulsion .

FI GURE 5 - Optical microscopy of the emu lsion prepared from Organoge: 4 (3%) in water (97%) . Water in oil emulsion (W/O).

Brief S u mmary of tho Invention

The cold or hot process preparation of cosmetic compositions, accord ing to the present invention, comprises two basic steps. The first step is the preparation of the organogels in wh ich liquid oils are structured by a mixture o ^c monoglycerides and waxes as structuring agents, which also have the addition of other components as polymers and polyol esters. The second step is the formation of cold process cosmetic compositions where emu lsions are- prepared by the add ition of water, aqueous solutions and other components, to the organogel . The em ulsions formed have superior sensory effect, chemical- physical characteristic and stability, to those currently produced by the classic technology of preparation with emu!sifiers prior art.

Detailed Descri ption of the Invention

The process, according to the present invention , is intended to cold or hot process cosmetic compositions, which include: oil in water (O/W), water in o;l (W/O) and lamel lar emulsion using a two-step process. The first step involves the preparation of the oily base that is structured by a mixture of compounds containing waxes, monoglycerides, polymers, and esters of polyols, in the form of organogel, U nlike conventional emu lsions, where the oil phase is in liquid form , according to the present invention , the oil phase is structured in the form of an organogel. I n a second step , named step of emulsification . the organogel formed is used as a base for the emulsion process . The emulsion is then formed by the audition of water, aqueous solutions and/or other components of the cosmetic composition , in the organogel .

The structuring agent is formed by a mixture of vegetable, animal, mineral or synthetic waxes , with monog iycerides, and their m ixtures, also from vegetable , an imal and/or synthetic sources . The organogels may also have in its composition , natu ral a nd/or synthetic polymers and polyois esters such as glycerol, xylito! , sorbitol and / or mannitol, as an improver i n the process of structu ring the emu lsion . The characteristics of the organogel formed will be defined by the proportion of each component, where the innovation is the incorporation of the oil phase not in the liquid form but as an organogel (solid ^¬ like material). This is done by a cold or hot process in a second step of the process. The synergism of the structuring agents and other components from the cosmetic composition, confer unique characteristics to the organogel and the resulting emulsions.

The concentration of structu ring agent and other components of organogel depend on the type of em ulsion being prepared. Typically, it varies from 0 , 2 to 70%. The same happens with the other components of the cosmetic composition . The concentration of wax in the organogel is in the range of 0 to 20%, preferably between 0.5% and 12% , or more precisely between 1 and 5% . The concentration of monogiycerides in the organogel is in the ra nge of 0 to 25%, preferably between 2 and 1 8%, or more precisely between 1 0 and 1 5%. The concentration of polymers in the organogel is in the range of 0 to 40%, preferably between 5% and 30% , or more precisely between 1 5 a nd 25%. The concentration of polyol in the organogel is in the range of 0 to 40% , preferably between 0. 1 and 30% , or more precisely between 0.2 and 20%.

The organic fluid being structured by structuring agents can be any type of vegetable , an imal , mineral or synthetic oil and its concentration may be in the range of 30 to 99% of organogel components.

The organogel is prepared by m ixing orga n ic fluio (oil) with the structuring agents. The oil is heated to between 60 and 95°C and structuring agents are added as well as other structural components such as polymers and polyol esters, and are mixed u ntil com plete dissolution. The organogel is formed during cooling of the mixture, The cooling process can be performed at cooling rates of -PC per hou r to 5°C per minute and temperatu res can vary between 25°C ( room temperature) and -5°C _; depending on the desired structu re. After the cooling process and formation of organogel , it is stored at temperatures between 5 and 40°C ,

The organogel formed is an oily base used to p ^r epare the emulsion in the second step of the process, in which water and other aqueous or non-aqueous ing redients, active or not. will be added and emu lsified . The resulting cosmetic compositions, and as described in the present invention, the oil phase of the emulsion is not in the liq uid form usually stabilized by an emu!sifier, but rather as an organogel , structured by a m ixtu re of structuring agents and which contains other components such as polymers and polyol esters. The concentrations of organogel water, aq ueous solutions and other components to be used in the cold or hot process of the emu lsion depend on the characteristics desired in the cosmetic final product.

The organogel prepared accord ing to the present invention can be applied in a variety of body care prod ucts or any cosmetic prod uct that requires formation of emu lsions , be them oi l-in-water (O/W). water in oil (W/O) or, lamella r emu lsions. These applications generate prod ucts with stability and sensory characteristics d ifferentiated . There is not a maximum or a m inimum concentration of the organogel to be used, but their concentration may vary from 0.1 to 20% , prefera bly between 0.5 and 1 0% or more precisely between 2 and 8%, The concentration should be chosen accord ing to the desired composition or viscosity of the final product.

Illustrative examp les, whether the organogels, mixtures of structu ral a nd other components of the cosmetic compositions that were formulated and processed u nder the conditions given below, serve to better describe the present invention . However, the data and proced ures presented merely reter to some forms of application of the present invention and should not be taken as limiting the scope thereof.

Examples

Example 1 . Organogel 1 Preparation

The Organogel 1 was prepared by combining high oleic sunflower oil (HOSO) as the organic fluid , that was structured with candelilla wax and glyceryl monostearate (monoglyceride) as structuring agents and Xylityl Sesqu icaprylate (polyol esters) and sod ium polyacrylate (polymer) as auxiliary compounds in stabi lizing the emulsion. The emulsion will be prepared using the organogel i n the second step of the process . The high oleic su nflower oil, cande!llla wax esters , xylitol, g lyceryl monostearate and sodium poiyacrylate a re mixed (500rpm) and heated (80°C) until the complete melting of all components. After incorporation of the ingred ients in the oil , the m ixture is stirred for 10 minutes at 1 ,4Q0rpm At the end of the process the mixture is cooled to room temperature (25°C) to allow the formation of organogel being stored at 8 ^C C .

I n the form u lation of Organogel 1 were used com ponents and concentrations listed in Table 1 ,

Example 1 A. Preparation of oil/water emulsions (O/W) using tne Organogel 1

The Organogel 1 was used to prepare oil in water emulsion by simply dispersing Organogel 1 in water with no heating . The emulsion was prepared by combining 3% of Organogel 1 with 97% of water. There is no need for hig h mechan ical agitation to achieve good dispersion and stability of the resulting em u lsion . The d ispersion of Organogel 1 in water forms an emulsion in which stability is conferred Dy the gelation of aqueous continuous phase and the oly dispersed phase. Gelation of the dispersed and continuous phases increases the viscosity of the medium retarding thereby agg lomeration of the dispersed phase and avoiding phase separation, which increases stability. The presence of the oily phase as organogel , and not as a liquid , can be confirmed by the presence of monog lyceride crystals (glyceryl monostearate) and wax (candelilla wax) within the oil globules, which is clearly shown in Fig ure 1 . The polarized lig ht microscopy was used to verify the presence of these crystals (monog lycerides and waxes inside the oil gelled g lobu les) which act as structu ri ng agents . These crystals, during the preparation process of the organogel in the cooling step, are organized forming a crystal lattice able to sustain the oil phase and to maintain the globule structu re.

It is well known that liquid oil, when emu lsified ;n water, is dispersed in small d roplets with a well defined rounded shape. I n this case, as can be seen in Figure 2 , the oil d roplet has not a rounded shape, further confirming its characteristic of a gel .

The viscosity of the em ulsion obtained was more than 5.1 (Tcps (Brookfieid LV. spi ndle TF) , with a uniform distribution of particle size. The distribution of the globu les of the emulsion formed with organogel can be seen in Figure 2, where the optical m icroscopy was used to verify the tyoe, d ispersion and stability of the emulsion. The application of Organogel 1 in water enables the formation of emulsions with excellent sensory attributes.

Example - I B. Preparation of a body lotion using Organogel 1

The fol lowing example describes the preparation of a cosmetic composition (body lotion) where Organogel 1 was applied at a concentration of 3%. Table 2 lists the ingredients used in the cosmetic formulation , In the process of obtaining the Iotion , the components in phase 2 were first combined with Organogel 1 (step 1 ) , This combination was made by a simple mixing of the two phases until the organogel had been completely dispersed, forming a homogeneous phase. Under moderate mechanical stirring (500 rpm) the third phase, which conta i ned water, and the fourth phase were incorporated into the mixture. The mixture was stirred for 1 5 min utes until the formation of a homogeneous emulsion .

Table 2 - Cosmetic composition (Body Iotion) prepared with Organogel 1

The oil in water emulsion obtained had high viscosity (> 5.10 cps), white color, and excellent gloss with a soft and pleasant feeling when applied to skin. The Organogel 1 proved to be effective when used to help the dispersion of an oil phase in water, even with an extra load of oil (phase 2) of 15%, The structure of Organogel 1 was suitable for forming a fine dispersion of globules. The emulsion stability tests revealed fully satisfactory results regarding viscosity and phi stability as shown in Table 3.

Table 3 - Stability of Viscosity and pH results of lotion prepared using

Example - 10. Preparation o:- a Sunscreen formulation using Organogel 1

The sunscreen, which formulation is described in Table 4, is another example where the Organogel 1 can be applied, in this case, the emulsion was prepared following tne procedure described in the previous example (IB), However, in this process, the components from phase 2, because they are solid, had to be melted and added, at a temperature of 40°C, to phase 1 that comprises the Organogel 1 The formation of the oil in water emulsion was made by a cold process (T - 25"C) with stirring. As described in Example 1 B, there is no need for high agitation. i able 4 - Cosmetic composition (sunscreen) prepared from Organogel 1

The results showed excellent physical and chemical stability of this cosmetic emulsion as shown in Table 5,

Table 5 - V.scosity and pH stability of a sunscreen formulation prepared using

Organogel ⁴ ,

Example - 1 D. Preparation o~ Hydroalcoholic gels using Organogel 1.

This example describes the preparation of hydroalcoholic gels using Organogel 1. The preparation of oil in water emulsion is made from the mixture of phases 1 and 2. according to the concentrations listed In Table 6. Phase 3 was subsequently incorporated, under mechanical stirring. The emulsion was prepared to evaluate the efficiency of the Organogel 1 to maintain the emulsion stable when different polar solvents such as ethanol, in concentrations of up to 30% are added to the emu lsion. The em ulsion formed was stable for 30 days at 45 " C for ethanol concentrations <30% .

Table 6 - Cosmetic composition (hydroalcoholic gel) prepared witn Org

The examples described above demonstrate the ability of Organogel 1 to form stable oil in water (O/W) emulsions. The emu lsions were read ily prepared at low temperature (room temperature), showed high stability, excellent appearance a nd h igh moisturizing effect.

Example - 2. Organogel 2 Preparation

Th is example describes the formulation of a prod uct which is referred to as Organogel 2 and has a similar composition to Organogel 1 (as seen in Table- 1 ) but with addition of 0,2% of poiyol esters (Xylityl Sequicaprylate) as T able 7, Candelilla wax, nigh oleic sunflower oil , g lyceryl monostearate and xylitol esters were mixed (500 rpm) and heated (80 ⁰ C) until complete melting of all components, Under high agitation, the sodium polyacrylate polymer was slowly added to the mixture. The mixture was cooled to permit ^f ormation of organogel .

Despite the smail concentration of xylitol esters (0.2%), it is observed that it has a significant infiuence on the formation and stabilization of cold process emulsions with characteristics superior to conventional emulsions including emulsions prepared with Organogel 1. The addition of xylitol esters is responsible for the formation of a structure different from that observed in Example 1, as can be seen in Figure 3, it was observed the presence of a lamellar structure, where the globules of organogel (disperse phase) in the emulsion are stabilized by a structure composed of layers of lamellar structuring. This reflects strongly and positively in the appearance of the resulting emulsion. Emulsions formed were whiter and less translucent.

Example - 2A. Preparation of Oil / Water (O / VV) Lamellar Emulsions from the

Organogel 2

The Organogel 2 was used to prepare an oil in water cold emulsion (O/W). merely by dispersing the Organogel 2 (3%) in water (97%). The dispersion of Organogel 2 in water forms an emulsion with differentiated characteristics. The globules of oil show to have inside, a lamellar structure, which results in an emulsion of high sensory quality, superior to traditional emulsions produced by a hot process .or even the other cold process emulsions, which use emulsifiers and oil liquid phases. Gelation of the dispersed and continuous phases increases the viscosity of the emulsion, thus slowing the agglomeration of the dispersed phase and. thereby, avoiding the phase separation. There was no need for high mechanical agitation to achieve good dispersion and stability of the oil phase in the aqueous phase.

The Organogel 2 can be applied to manufacture a wide variety of body-care products, cosmetics or any other product that require the formation of oil in water emulsion. These applications generate products with superior sensory characteristics when compared to other cold process emulsions. There is not maximum or minimum concentration of Organoge 2 to be dispersed in water. It is recommended between 3 - 5% for lotions with viscosity of about 30,000 to 70.000cps. Example - 2B. Preparation of Moisturizing Lotion using Organogel 2

The cosmetic composition of a moisturizing lotion, where Organogel 2 was applied, is shown in Table 8 In the process of obtaining the lotion, the components of phase 2 were primarily combined with the phase 1 (organogel). This combination was made by a simple mixing (low shear) of the two phases, with a complete dispersion of the organogel in the oil phase, to form a homogeneous phase. Under moderate mechanical stirring (500 rpm) stages 3 and 4 were Incorporated into the mixture. The mixture was stirred continuously until the formation of a homogeneous emulsion (15 minutes).

The emulsion formed presented adeguate viscosity for this type of product, white color, excellent gloss and a smooth sensory touch when applied to the skin. Despite the low concentration of xylitol esters in Organogel 2. its addition contributes to improve and facilitate oil dispersion as well as the appearance and sensory effect of the resulting emulsion. The determination of emulsion stability proved fully satisfactory results regarding the appearance, viscosity and pH, as shown in Table 9.

Table 8 - Composition cosmetics (Lotion) prepared with 2 Organogel

Table 9_- Viscosjty_and pH stability of the lotion prepared from Organogel 2 INITIAL VISCOSITY (cps) 30,5'T

VISCOSITY AT ROOM TEMPERATURE (30 DAYS) 26,650

Example - 3. Organogel 3 Preparation

The organogel prepared by combining the ingredients described in Table 10 will be referred to as Organogel 3. The preparation of Organogel 3 was also performed as described in Examples 1 and 2. The difference, in this case, is the concentration of the polyol esters (Xylityl Sesquicaprylate), It Is Important to mention that, when the concentration of esters of xylitol is increased or decreased in the formulation, the proportion of total, or part, of the components can be changed. The formulation of Organogel 3 was developed for the preparation and stabilization of lamellar cold process emulsions as described in the following examples.

Example - 3A Preparation of Lamellar Oil/Water (O/W) Emulsions using the Organogel 3

The ability of Organogel 3 in developing lamellar emulsions was demonstrated. In this example, 3% of Organogel 3 and 97% water were mixed slowly uncer moderate agitation (500 rpm). After the emulsion being formed, it was homogenized for 10 minutes. With the addition of Xylityl Sesquicaprylate to the organogel, it was observed the formation of an oil in water emulsion, where the dispersed cells of trie organogel showed a different form of structure, a lamellar structure within the globule, as seen in Example 2. This different way of structuring, conferred a higher quality than the emulsion formed in terms of dispersion and sensory effect. This behavior was observed when the concentration of Xylityl Sesquicap ryiate ranged from 2 to 40% in the organogel form ulation . However, it also was noticed that, when a hig h concentrations of Xylityl Sesqu icapryiate (20-40%) is used in the formulation of O rganogel 3 and this is dispersed in a greater concentration of oil phase, lamellar emulsions are generated and the oil phase (organogel) is retained withi n lamellae , as seen in F igu re -O

This organogel , as well as ail others previously described , can be used for the preparation of a number of hygiene products and body care, as in the example described below.

Example - 3B. Preparation of Facial Cream using Organoqel 3

The com position described in Table 1 1 illustrates the use of Organogel 3 as the base i n the preparation of a facial cream . As described in Example 1 B the components of phase 2 were previously combined with phasel , as well as the components of phase 3 and 4. The two mixtures were then combined and mixed under mechan ical stirring . The process was conducted at room temperature.

Table 1 1 - Cosmetic Composition (Facial Cream) prepared with Organogel 3

The lamellar emulsion generated by the presence of Organogel 3, which contained high concentration Xyiityl Sesquicapryiate, resulted in a new microstructure of the emulsions. Unlike the conventional microstructure of oil in water emulsions, in this case the oil phase, in the form of an organogel, was located on the external interface of the globule forming a lamellar structure. This is part of a more complex definition, where the oil phase is surrounded by several layers containing the structuring agent. The main characteristics of the emulsion prepared with Organogel 3 are, the appearance and the sensory effect (with a no tack touch). Table 12 shows the results of the viscosity and the pH during stability tesi of the lamellar emulsion formed in the facial cream formulation. Results were considered satisfactory to such cosmetic composition.

Table 12 - Viscosity and pH stability of lotion Drep red from Organogel 3.

Example - 4. Preparation of Organogel 4

The combination and concentrations of ingredients listed in Table 13 will be referred to as Organogel 4, The organogel ^' was specially formulated for preparing water in oil (W/O) cold process emulsions, by incorporating in the organogel the surfactant Polyglycerol Polyricinoleate. a polyol ester. This organogel was prepared just as illustrated previously, except for the addition of the Polyglycerol Polyricinoleate that happens in the end of the process. The organogel obtained had excellent texture and a fine monoglycerlde and wax crystallization.

The ability of the Organogel 4 in forming water-in-oii (W/O) emulsions is shown in Examples 4A and 4B described below.

Example - 4A. Water in oii emulsion (W/O) prepared using Organogel 4

in this example, 3% of Organogel 4 and 97% of water were mixed under high agitation (1400 rpm), After the emulsion being formed it was homogenized for 10 minutes to ensure good dispersion. Given the stnail concentration of Organogel 4 and hence a lower concentration of nonpoiar phase (continuous phase of the emulsion water in oil), the emulsion formed had a high viscos.ty. being greater than 3 105 cps (Brookfield LV - spindle TF). Tine emulsion formed was characterized by a unique touch combined with a moisturizing effect, a refreshing feeling due to water in gel form and a final touch of softness without being overly oily. The combination of water and Organogel 4 creates better distribution of tne water droplets which also help to increase the stability of the emulsion. The process was conducted at room temperature (cold process), and the microstructure of the emulsion is shown in Figure 5. that is characteristic of wate ^r m oil emulsion

Example - 4B. Preparation of Sunscreen SPF 30 using 4 Organogel

The Organogel 4 was used as the base for the preparation of an

SPF 30 sunscreen whose formulation is described in Table 14. In their preparation, the components of phases 2 were first combined with the first phase. Phase 2 was melted and cooled to 40°C before incorporation of phase 1. Under high mechanical stirring (1400 rpm) phase 3 was slowly incorporated into the mixture.

Table 14 - Cosmetics composition (Sunscreen SPF 30) prepared with

I + C12-C15 A!kyl Benzoate 1.0

Octyl Methoxycinamate 8.0

Uvinu) T-150 4,0

Tmoso'b S 3.0

Parsol TX 50 AB 6,0

Preservative 0.05

PHASE 3

Glycerin 2,0

Water p. 100

Tinosorb M 2.0

The sunscreen prepared with Organogel 4 showed initial viscosity of 155,500 cps. After 30 days of storage at room temperature the viscosity remained at 148,750 cps.